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Reactions of 2,6-pyridinedicarboxylic acid or 2,6-dibromomethyl pyridine with 5-(4-hydroxyphenyl)-10,15,20-triphenyl porphyrin, 5-(4-aminophenyl)-10,15,20 triphenyl porphyrin gave three novel bridged diporphyrins 3-5, respectively.

通过将2,6-吡啶二羧酸或2,6-二溴甲基吡啶分别与5-(4-羟基苯基)-10,15,20-三苯基卟啉(1)和5-(4-氨基苯基)-10,15,20-三苯基卟啉(2)反应,合成了3种新型的双卟啉化合物3~5。

From the UV spectra, it can be found that the aromaticity of acenaphthenyl groups in C_2 gum is the largest. But there are 30 carbon atoms in the conjugated structure of condensed aromatics in C_1 gum and C_3 gum, while 28 carbon atoms in acenaphthenyl groups in C_2 gum.

但是,在C_1胶、C_2胶和C_3胶三者中,C_1胶侧链上的四苯基苯基和C_3胶侧链上的菲式多苯基苯基都含有30个碳原子,而C_2胶侧链上的苊式多苯基苯基含有28个碳原子,比前面二者小2个碳原子,理应其芳香性在三者之中最小,但事实却恰恰相反。

While all the phenyl groups in tetraphenylphenyl groups or benzophenanthrene groups are not coplanar. At the same time, by density function theory, the electronic energy gap between HOMO and LUMO frontier molecular orbitals of condensed aromatics are calculated and the Eg of acenaphthenyl groups in C_2 gum is the smallest, which explains the reason why C_2 gum has the best radiation protection effects.

利用甲基三氯硅烷和溴苯的格氏反应合成了甲基苯基二氯硅烷,用核磁分析证实了格氏反应中高沸点副产物为甲基二苯基氯硅烷;通过甲基苯基二氯硅烷和二甲基二氯硅烷的共水解,再裂解而制得含Me_2SiO链节的甲基苯基环硅氧烷混合物,进而利用碱胶开环聚合得到甲基苯基硅橡胶生胶;也可通过甲基苯基二氯硅烷水解所得甲基苯基环硅氧烷D_3~(3Ph、D_4~(4Ph_)与D_4开环聚合制得甲基苯基硅橡胶生胶。

So, by the Diels-Alder reaction of tetraphenylcyclopentadienone, acenaphthenecyclone and benzophenanthrenecyclone with the vinyl groups in C gum, three kinds of polymethylvinylsilicone oil with condensed aromatics are synthesized respectively: polymethylvinylsilicone oil with tetraphenylphenyl groups (called C_1 gum for short), polymethylvinylsilicone oil with acenaphthenyl groups (C_2 gum) and polymethylvinylsilicone oil with benzophenanthrene groups (C3 gum).

根据此原则,利用四苯基环戊二烯酮、苊式环戊二烯酮和菲式环戊二烯酮与C胶上的乙烯基进行Diels—Alder反应,分别合成了三种含稠环基团的乙烯基硅油:四苯基苯基乙烯基硅油(C_1胶),苊式多苯基苯基乙烯基硅油(C_2胶)和菲式多苯基苯基乙烯基硅油(C_3胶),并根据~1HNMR谱图上不同氢原子的积分面积计算了三种胶中稠环基团和乙烯基的含量。

Seven Schiff bases of N-(4-hydroxyphenylmethylene)-1-naphthylamine, N-(4-hydroxyphenylmethylene)-p-methoxyaniline, N-(4-hydroxyphenylmethylene)-benzylamine, N-(4-hydroxy-3-methoxyphenylmethylene) furfurylamine, N-(4-hydroxy-3-methoxyphenyl methylene)-p-methylaniline, N-(4-hydroxy-3-methoxyphenylmethylene)-p-methoxyaniline and N-salicylidene-4-aminoantipyrine were first synthesized by the one step solid phase reactions between aromatic aldehydes with phenolic hydroxyl and amines at room temperature without solvent.

分别以带酚羟基的芳醛与胺类反应,首次通过室温固相反应一步合成了N-(4-羟基苯基亚甲基)-1-萘胺、N-(4-羟基苯基亚甲基)-对甲氧基苯胺、N-(4-羟基苯基亚甲基)-苄胺、N-(4-羟基-3-甲氧基苯基亚甲基)糠胺、N-(4-羟基-3-甲氧基苯基亚甲基)-对甲苯胺、N-(4-羟基-3-甲氧基苯基亚甲基)-对甲氧基苯胺和N-亚水杨基-4-氨基安替比林7种Schiff碱,反应15min完成,产率均超过90%。

In this paper four watery UV photoinitiators were studied and synthesized through a four-step process. They were l-(4-aminophenyl)-2-piperidino-1-propanone dihydrochloride, 1 -(4-aminophenyl)-2-morpholino-1 -propanone dihydrochloride, 1 -(4-aminophenyl)-2-diethylamino-1 -propanone dihydrochloride, 1 -(4-aminophenyl)-2-burylamino-1-propanone dihydrochloride, which have not been reported in any literatures till now.

本文通过四步反应合成了目前未见报道的四种水性紫外光引发剂:1-(4-氨基苯基)-2-哌啶基-1-丙酮盐酸盐、1-(4-氨基苯基)-2-吗啉基-1-丙酮盐酸盐,1-(4-氨基苯基)-2-二乙胺基-1-丙酮盐酸盐、1-(4-氨基苯基)-2-正丁胺基-1-丙酮盐酸盐。

Two novel pyrazolone derivatives 2-ethylamino-6H-5-(1-phenyl-3-methyl/phenyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine (PMCP-ETSC/DPCP-ETSC) containing NNS six-membered heterocycles were synthesized by the condensation reaction of 1-phenyl-3-methyl/phenyl-4-chloroacetyl-pyrazolone-5 with 4-ethyithiosemicarbazide. The title compounds were characterized by elemental analysis, IR, 1H NMR, 13C NMR and single-crystal X-ray diffraction.

利用1-苯基-3-甲基/苯基-4-氯乙酰基-吡唑啉酮-5与4-乙基氨基硫脲发生缩合反应,生成了2个新的双杂环化合物2-乙氨基-6H-5-(1-苯基-3-甲基/苯基-5-吡唑啉酮-4-基)-1,3,4-噻二嗪(PMCP-ETSC/DPCP-ETSC),并对其进行元素分析、红外光谱、核磁共振表征和晶体结构分析。

The preliminary bioassays indicated that, at 500 g/mL, 1-(o-tolyl-4-(4-chloro-3-ethyl-1-methylpyrazol-5-ylcarbonyl)semicarbazide (4g) and 1-(2,4-dimethyl- phenyl)-4-(4-chloro-3-ethyl-1-methylpyrazol-5-ylcarbonyl)semicarbazide (4k) showed inhibitory activities 90% and 80% against Blumeria graminis, respectively; and at 25 g/mL, 4-phenyl-4-(4-chloro-3-ethyl-1- methylpyrazol-5-ylcarbonylsemicarbazide (4c) showed inhibitory activity 70.1% against Botrytis cinerea and 1-2-nitro-phenyl-4-(4-chloro-3-ethyl-1-methylpyrazol-5-ylcarbonylsemicarbazide (4d) showed inhibi-tory activitiy 51.3% against Pyricularia oryzae.

初步生物活性实验结果表明,在500 mg/mL浓度下,化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2-甲基苯基)氨基脲(4g), 1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2,4-二甲基苯基)氨基脲(4k)对小麦白粉病菌的抑制率分别达到90%和80%;在25 mg/mL浓度下,化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-苯基氨基脲(4c)对黄瓜灰霉病菌的抑制率达到70.1%;化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-苯基氨基脲(4c)和1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2-硝基苯基)氨基脲(4d)对稻瘟病菌的抑制率均达到51.3%。

A compound of formula wherein R1 is hydrogen, halo or methoxy; R2 is hydrogen, halo, methyl, ethyl or methoxy; R3 is carboxy, tetrazolyl, or -CONHSO2R where R is methyl, ethyl, phenyl, 2,5-dimethylisoxazolyl or trifluoromethyl; T is -CH2- or -SO2-; and ring A is 3-chlorophenyl, 4-chlorophenyl, 3-trifluoromethylphenyl, 3,4-dichlorophenyl, 3,4-difluorophenyl, 3-fluoro-4-chlorophenyl, 3-chloro-4-fluorophenyl or 2,3-dichloropyrid-5-yl; or a pharmaceutically acceptable salt or prodrug thereof, as well as pharmaceutical compositions containing them are described and claimed.

本发明涉及一种式化合物,其中R 1 是氢原子、卤素或甲氧基;R 2 是氢原子、卤素、甲基、乙基或甲氧基;R 3 是羧基、四唑基或-CONHSO 2 R 4 ,其中R 4 是甲基、乙基、苯基、2,5-二甲基异∴唑基或三氟甲基;T是-CH 2 -或-SO 2 -;环A是3-氯苯基、4-氯苯基、3-三氟甲基苯基、3,4-二氯苯基、3,4-二氟苯基、3-氟-4-氯苯基、3-氯-4-氟苯基或2,3-二氯吡啶-5-基;或其药用允许的盐或前药,还包括所阐述和要求权利的含有它们的药用组合物。

The method comprises: adding 4-(3,4-dichlorophenyl)-1-tetralone and solvent at a ratio of 1:(3-4) into a three-necked flask with a stirrer, heating under stirring until 4-(3,4-dichlorophenyl)-1-tetralone is completely dissolved, heating to 60-100 deg.C, refluxing for 0.5-2 h, cooling the filtrate to -5-10 deg.C, filtering, recrystallizing to obtain refined 4-(3,4-dichlorophenyl)-1-tetralone, and drying at 40-80 deg.C to obtain dry 4-(3,4-dichlorophenyl)-1-tetralone.

该方法的步骤是:在带搅拌的三颈瓶中依次加入4-(3,4-二氯苯基)-1-萘满酮和溶剂,溶剂与4-(3,4-二氯苯基)-1-萘满酮的L∶W为3~4∶1,将上述4-(3,4-二氯苯基)-1-萘满酮及混合精制溶剂搅拌下升温,使4-(3,4-二氯苯基)-1-萘满酮全部溶解,升温至60~100℃,回流0.5-2h;滤液用冰水冷却至-5~10℃,过滤,所得物料再用上述方法进行一次重结晶得到精品4-(3,4-二氯苯基)-1-萘满酮,40~80℃干燥后即得到干品4-(3,4-二氯苯基)-1-萘满酮。

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